Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dr Edit Tshuva' _publ_contact_author_address ; Department of Inorganic Chemistry Hebrew University of Jerusalem Givat Ram Campus Jerusalem 91904 ISRAEL ; _publ_contact_author_email TSHUVA@CHEM.CH.HUJI.AC.IL _publ_section_title ; Distinctive Structural Features of Hydroxyamino-1,3,5-Triazine Ligands Leading to Enhanced Hydrolytic Stability of their Titanium Complexes ; loop_ _publ_author_name 'Dani Peri' 'Jacob S. Alexander' 'Edit Tshuva' 'Artem Melman' data_danip1m _database_code_depnum_ccdc_archive 'CCDC 604238' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H56 N12 O4 Ti, 2(C4 H10 O)' _chemical_formula_sum 'C42 H76 N12 O6 Ti' _chemical_formula_weight 893.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9542(12) _cell_length_b 12.6502(12) _cell_length_c 17.5705(17) _cell_angle_alpha 79.126(2) _cell_angle_beta 80.599(2) _cell_angle_gamma 66.344(2) _cell_volume 2378.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.247 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 964 _exptl_absorpt_coefficient_mu 0.237 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.5766 _exptl_absorpt_correction_T_max 0.9790 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13465 _diffrn_reflns_av_R_equivalents 0.0420 _diffrn_reflns_av_sigmaI/netI 0.1232 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9135 _reflns_number_gt 6170 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0803P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9135 _refine_ls_number_parameters 558 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1348 _refine_ls_R_factor_gt 0.0916 _refine_ls_wR_factor_ref 0.2024 _refine_ls_wR_factor_gt 0.1827 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7076(4) 0.7627(4) 0.4575(2) 0.0145(9) Uani 1 1 d . . . C2 C 0.7677(4) 0.5743(4) 0.5087(2) 0.0157(9) Uani 1 1 d . . . C3 C 0.6785(4) 0.6321(4) 0.3968(2) 0.0143(9) Uani 1 1 d . . . C4 C 0.6857(4) 0.9353(4) 0.5142(2) 0.0189(10) Uani 1 1 d . . . H4A H 0.6011 0.9708 0.5374 0.028 Uiso 1 1 calc R . . H4B H 0.7182 0.9961 0.4940 0.028 Uiso 1 1 calc R . . H4C H 0.7364 0.8795 0.5539 0.028 Uiso 1 1 calc R . . C5 C 0.6184(4) 0.5259(4) 0.3155(3) 0.0210(10) Uani 1 1 d . . . H5A H 0.6553 0.4580 0.3539 0.031 Uiso 1 1 calc R . . H5B H 0.6610 0.5107 0.2638 0.031 Uiso 1 1 calc R . . H5C H 0.5315 0.5405 0.3153 0.031 Uiso 1 1 calc R . . C6 C 0.8550(4) 0.5156(4) 0.6346(2) 0.0233(11) Uani 1 1 d . . . H6 H 0.8389 0.6007 0.6245 0.028 Uiso 1 1 calc R . . C7 C 0.7747(4) 0.4981(5) 0.7077(3) 0.0280(11) Uani 1 1 d . . . H7A H 0.7877 0.4146 0.7204 0.034 Uiso 1 1 calc R . . H7B H 0.6874 0.5427 0.6987 0.034 Uiso 1 1 calc R . . C8 C 0.8039(4) 0.5377(5) 0.7755(3) 0.0295(12) Uani 1 1 d . . . H8A H 0.7542 0.5204 0.8233 0.035 Uiso 1 1 calc R . . H8B H 0.7815 0.6231 0.7653 0.035 Uiso 1 1 calc R . . C9 C 0.9391(5) 0.4776(5) 0.7880(3) 0.0333(13) Uani 1 1 d . . . H9A H 0.9584 0.3937 0.8061 0.040 Uiso 1 1 calc R . . H9B H 0.9564 0.5111 0.8291 0.040 Uiso 1 1 calc R . . C10 C 1.0216(4) 0.4909(5) 0.7135(3) 0.0317(12) Uani 1 1 d . . . H10A H 1.0121 0.5735 0.7000 0.038 Uiso 1 1 calc R . . H10B H 1.1084 0.4437 0.7228 0.038 Uiso 1 1 calc R . . C11 C 0.9909(4) 0.4528(5) 0.6462(3) 0.0270(11) Uani 1 1 d . . . H11A H 1.0117 0.3676 0.6562 0.032 Uiso 1 1 calc R . . H11B H 1.0405 0.4696 0.5981 0.032 Uiso 1 1 calc R . . C12 C 0.8430(4) 0.3654(4) 0.5643(3) 0.0220(10) Uani 1 1 d . . . H12 H 0.8881 0.3222 0.6109 0.026 Uiso 1 1 calc R . . C13 C 0.7299(4) 0.3363(4) 0.5761(3) 0.0275(11) Uani 1 1 d . . . H13A H 0.6833 0.3708 0.5298 0.033 Uiso 1 1 calc R . . H13B H 0.6763 0.3699 0.6219 0.033 Uiso 1 1 calc R . . C14 C 0.7669(5) 0.2042(4) 0.5887(3) 0.0360(13) Uani 1 1 d . . . H14A H 0.8056 0.1710 0.6381 0.043 Uiso 1 1 calc R . . H14B H 0.6929 0.1859 0.5929 0.043 Uiso 1 1 calc R . . C15 C 0.8561(5) 0.1498(5) 0.5219(4) 0.0431(15) Uani 1 1 d . . . H15A H 0.8134 0.1754 0.4740 0.052 Uiso 1 1 calc R . . H15B H 0.8832 0.0640 0.5335 0.052 Uiso 1 1 calc R . . C16 C 0.9688(4) 0.1820(4) 0.5073(3) 0.0360(13) Uani 1 1 d . . . H16A H 1.0180 0.1476 0.5524 0.043 Uiso 1 1 calc R . . H16B H 1.0205 0.1494 0.4607 0.043 Uiso 1 1 calc R . . C17 C 0.9314(4) 0.3137(4) 0.4949(3) 0.0271(11) Uani 1 1 d . . . H17A H 0.8909 0.3476 0.4463 0.033 Uiso 1 1 calc R . . H17B H 1.0051 0.3327 0.4901 0.033 Uiso 1 1 calc R . . C18 C 0.6456(4) 0.9903(4) 0.1560(2) 0.0184(10) Uani 1 1 d . . . C19 C 0.5090(5) 1.1359(4) 0.0823(3) 0.0248(11) Uani 1 1 d . . . C20 C 0.4418(4) 1.0637(4) 0.1992(2) 0.0167(10) Uani 1 1 d . . . C21 C 0.8722(4) 0.8998(5) 0.1370(3) 0.0311(12) Uani 1 1 d . . . H21A H 0.8635 0.9473 0.0857 0.047 Uiso 1 1 calc R . . H21B H 0.9188 0.8177 0.1306 0.047 Uiso 1 1 calc R . . H21C H 0.9157 0.9249 0.1680 0.047 Uiso 1 1 calc R . . C22 C 0.2338(4) 1.1204(4) 0.2719(3) 0.0293(12) Uani 1 1 d . . . H22A H 0.2192 1.1696 0.3123 0.044 Uiso 1 1 calc R . . H22B H 0.1896 1.0681 0.2887 0.044 Uiso 1 1 calc R . . H22C H 0.2046 1.1696 0.2234 0.044 Uiso 1 1 calc R . . C23 C 0.5784(6) 1.2122(5) -0.0491(3) 0.0398(15) Uani 1 1 d . . . H23 H 0.5301 1.2734 -0.0893 0.048 Uiso 1 1 calc R . . C24 C 0.6300(5) 1.1086(5) -0.0893(4) 0.0514(16) Uani 1 1 d . . . H24A H 0.5621 1.0911 -0.1020 0.062 Uiso 1 1 calc R . . H24B H 0.6797 1.0412 -0.0539 0.062 Uiso 1 1 calc R . . C25 C 0.7108(5) 1.1249(5) -0.1648(3) 0.0430(15) Uani 1 1 d . . . H25A H 0.7540 1.0496 -0.1854 0.052 Uiso 1 1 calc R . . H25B H 0.6585 1.1810 -0.2045 0.052 Uiso 1 1 calc R . . C26 C 0.8029(6) 1.1692(6) -0.1493(4) 0.0589(18) Uani 1 1 d . . . H26A H 0.8639 1.1063 -0.1173 0.071 Uiso 1 1 calc R . . H26B H 0.8471 1.1873 -0.1996 0.071 Uiso 1 1 calc R . . C27 C 0.7501(5) 1.2745(5) -0.1091(3) 0.0376(14) Uani 1 1 d . . . H27A H 0.7017 1.3417 -0.1451 0.045 Uiso 1 1 calc R . . H27B H 0.8178 1.2917 -0.0958 0.045 Uiso 1 1 calc R . . C28 C 0.6684(4) 1.2609(5) -0.0353(3) 0.0330(12) Uani 1 1 d . . . H28A H 0.7199 1.2082 0.0058 0.040 Uiso 1 1 calc R . . H28B H 0.6230 1.3376 -0.0170 0.040 Uiso 1 1 calc R . . C29 C 0.3573(5) 1.2952(5) 0.0030(3) 0.0421(15) Uani 1 1 d . . . H29 H 0.3081 1.2814 0.0528 0.051 Uiso 1 1 calc R . . C30 C 0.3022(6) 1.2671(6) -0.0577(4) 0.0546(18) Uani 1 1 d . . . H30A H 0.3550 1.2655 -0.1075 0.066 Uiso 1 1 calc R . . H30B H 0.3002 1.1885 -0.0415 0.066 Uiso 1 1 calc R . . C31 C 0.1751(6) 1.3533(5) -0.0703(4) 0.0573(19) Uani 1 1 d . . . H31A H 0.1188 1.3414 -0.0246 0.069 Uiso 1 1 calc R . . H31B H 0.1490 1.3377 -0.1163 0.069 Uiso 1 1 calc R . . C32 C 0.1619(6) 1.4821(6) -0.0830(4) 0.062(2) Uani 1 1 d . . . H32A H 0.2083 1.4988 -0.1327 0.075 Uiso 1 1 calc R . . H32B H 0.0746 1.5344 -0.0854 0.075 Uiso 1 1 calc R . . C33 C 0.2126(5) 1.5021(5) -0.0148(3) 0.0374(13) Uani 1 1 d . . . H33A H 0.2103 1.5826 -0.0240 0.045 Uiso 1 1 calc R . . H33B H 0.1589 1.4946 0.0335 0.045 Uiso 1 1 calc R . . C34 C 0.3414(5) 1.4186(5) -0.0031(3) 0.0422(15) Uani 1 1 d . . . H34A H 0.3974 1.4358 -0.0472 0.051 Uiso 1 1 calc R . . H34B H 0.3650 1.4307 0.0451 0.051 Uiso 1 1 calc R . . C35 C 0.5373(5) 0.2899(5) 0.2264(3) 0.0333(13) Uani 1 1 d . . . H35A H 0.4552 0.2882 0.2265 0.040 Uiso 1 1 calc R . . H35B H 0.6001 0.2127 0.2168 0.040 Uiso 1 1 calc R . . C36 C 0.5543(5) 0.3827(5) 0.1642(3) 0.0424(15) Uani 1 1 d . . . H36A H 0.4890 0.4582 0.1727 0.064 Uiso 1 1 calc R . . H36B H 0.5507 0.3644 0.1131 0.064 Uiso 1 1 calc R . . H36C H 0.6342 0.3861 0.1661 0.064 Uiso 1 1 calc R . . C37 C 0.5267(5) 0.2358(4) 0.3614(3) 0.0374(14) Uani 1 1 d . . . H37A H 0.5844 0.1554 0.3547 0.045 Uiso 1 1 calc R . . H37B H 0.4420 0.2396 0.3636 0.045 Uiso 1 1 calc R . . C38 C 0.5447(5) 0.2676(5) 0.4352(3) 0.0460(16) Uani 1 1 d . . . H38A H 0.6265 0.2699 0.4309 0.069 Uiso 1 1 calc R . . H38B H 0.5370 0.2094 0.4790 0.069 Uiso 1 1 calc R . . H38C H 0.4823 0.3444 0.4439 0.069 Uiso 1 1 calc R . . C39 C 0.9300(7) 0.2013(7) 0.1383(4) 0.077(2) Uani 1 1 d . . . H39A H 0.9455 0.2649 0.1542 0.092 Uiso 1 1 calc R . . H39B H 0.8427 0.2315 0.1284 0.092 Uiso 1 1 calc R . . C40 C 1.0065(7) 0.1672(6) 0.0672(4) 0.072(2) Uani 1 1 d . . . H40A H 1.0926 0.1464 0.0749 0.108 Uiso 1 1 calc R . . H40B H 0.9821 0.2322 0.0250 0.108 Uiso 1 1 calc R . . H40C H 0.9966 0.1000 0.0537 0.108 Uiso 1 1 calc R . . C41 C 0.8779(7) 0.1348(7) 0.2681(4) 0.099(3) Uani 1 1 d . . . H41A H 0.7908 0.1724 0.2572 0.119 Uiso 1 1 calc R . . H41B H 0.8979 0.1904 0.2907 0.119 Uiso 1 1 calc R . . C42 C 0.8955(6) 0.0301(6) 0.3236(3) 0.067(2) Uani 1 1 d . . . H42A H 0.8773 -0.0255 0.3008 0.100 Uiso 1 1 calc R . . H42B H 0.8403 0.0500 0.3711 0.100 Uiso 1 1 calc R . . H42C H 0.9807 -0.0049 0.3364 0.100 Uiso 1 1 calc R . . N1 N 0.6877(3) 0.8757(3) 0.45160(19) 0.0179(8) Uani 1 1 d . . . N2 N 0.7591(3) 0.6821(3) 0.51536(19) 0.0152(8) Uani 1 1 d . . . N3 N 0.7275(3) 0.5436(3) 0.45109(19) 0.0151(8) Uani 1 1 d . . . N4 N 0.6293(3) 0.6260(3) 0.3356(2) 0.0187(8) Uani 1 1 d . . . N5 N 0.6683(3) 0.7426(3) 0.39584(18) 0.0135(8) Uani 1 1 d . . . N6 N 0.7531(3) 0.9136(3) 0.1759(2) 0.0225(9) Uani 1 1 d . . . N7 N 0.6280(4) 1.0651(3) 0.08971(19) 0.0218(9) Uani 1 1 d . . . N8 N 0.4117(4) 1.1417(3) 0.1355(2) 0.0213(9) Uani 1 1 d . . . N9 N 0.3626(3) 1.0529(3) 0.2594(2) 0.0215(9) Uani 1 1 d . . . N10 N 0.5559(3) 0.9847(3) 0.21119(18) 0.0147(8) Uani 1 1 d . . . N11 N 0.8219(3) 0.4878(3) 0.5653(2) 0.0201(8) Uani 1 1 d . . . N12 N 0.4841(4) 1.2116(4) 0.0150(2) 0.0308(11) Uani 1 1 d . . . O1 O 0.6166(3) 0.9445(3) 0.39144(16) 0.0193(7) Uani 1 1 d . . . O2 O 0.5739(3) 0.7319(2) 0.29060(16) 0.0189(7) Uani 1 1 d . . . O3 O 0.7495(3) 0.8487(3) 0.24881(16) 0.0202(7) Uani 1 1 d . . . O4 O 0.4151(3) 0.9663(3) 0.31971(16) 0.0191(7) Uani 1 1 d . . . O5 O 0.5487(3) 0.3155(3) 0.29809(17) 0.0223(7) Uani 1 1 d . . . O6 O 0.9526(3) 0.1083(3) 0.1989(2) 0.0442(10) Uani 1 1 d . . . Ti1 Ti 0.59109(7) 0.87152(7) 0.31073(4) 0.0144(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.017(2) 0.014(2) 0.013(2) -0.0011(18) 0.0036(17) -0.0095(19) C2 0.013(2) 0.018(2) 0.015(2) 0.0012(18) 0.0016(17) -0.0076(19) C3 0.018(2) 0.013(2) 0.014(2) -0.0033(18) 0.0025(17) -0.0086(19) C4 0.020(2) 0.016(2) 0.023(2) -0.009(2) -0.0009(19) -0.008(2) C5 0.026(3) 0.016(2) 0.025(2) -0.003(2) -0.005(2) -0.011(2) C6 0.030(3) 0.019(3) 0.020(2) -0.002(2) -0.008(2) -0.005(2) C7 0.021(3) 0.031(3) 0.030(3) -0.008(2) -0.002(2) -0.007(2) C8 0.030(3) 0.031(3) 0.021(2) -0.007(2) -0.002(2) -0.005(2) C9 0.033(3) 0.042(3) 0.023(3) -0.007(2) -0.006(2) -0.011(3) C10 0.026(3) 0.042(3) 0.028(3) 0.000(2) -0.010(2) -0.014(3) C11 0.023(3) 0.037(3) 0.024(2) -0.004(2) 0.000(2) -0.016(2) C12 0.025(3) 0.014(2) 0.023(2) 0.004(2) -0.006(2) -0.004(2) C13 0.023(3) 0.020(3) 0.039(3) -0.003(2) -0.004(2) -0.007(2) C14 0.030(3) 0.024(3) 0.055(3) 0.003(3) -0.008(3) -0.013(2) C15 0.032(3) 0.019(3) 0.081(4) -0.010(3) -0.015(3) -0.007(2) C16 0.023(3) 0.020(3) 0.062(4) -0.009(3) -0.006(3) -0.003(2) C17 0.024(3) 0.023(3) 0.037(3) -0.006(2) -0.005(2) -0.010(2) C18 0.021(2) 0.019(2) 0.020(2) -0.0032(19) -0.0064(19) -0.010(2) C19 0.041(3) 0.024(3) 0.022(2) 0.005(2) -0.017(2) -0.023(2) C20 0.026(3) 0.012(2) 0.020(2) -0.0010(19) -0.0074(19) -0.013(2) C21 0.024(3) 0.032(3) 0.037(3) -0.010(2) 0.004(2) -0.011(2) C22 0.018(3) 0.031(3) 0.035(3) -0.010(2) -0.005(2) -0.002(2) C23 0.071(4) 0.043(4) 0.021(3) 0.002(3) -0.008(3) -0.039(3) C24 0.037(3) 0.044(4) 0.081(4) -0.031(4) 0.010(3) -0.021(3) C25 0.051(4) 0.032(3) 0.050(3) -0.016(3) -0.013(3) -0.013(3) C26 0.054(4) 0.057(5) 0.061(4) -0.021(4) 0.015(3) -0.019(4) C27 0.053(4) 0.036(3) 0.032(3) 0.004(3) -0.013(3) -0.025(3) C28 0.025(3) 0.028(3) 0.049(3) -0.015(3) 0.003(2) -0.011(2) C29 0.057(4) 0.035(3) 0.042(3) 0.027(3) -0.036(3) -0.028(3) C30 0.051(4) 0.050(4) 0.080(5) -0.025(4) -0.022(4) -0.025(3) C31 0.056(4) 0.045(4) 0.090(5) 0.015(4) -0.043(4) -0.035(3) C32 0.047(4) 0.046(4) 0.099(5) -0.012(4) -0.042(4) -0.008(3) C33 0.034(3) 0.046(4) 0.041(3) -0.010(3) -0.005(3) -0.023(3) C34 0.032(3) 0.053(4) 0.054(3) -0.033(3) -0.002(3) -0.018(3) C35 0.024(3) 0.031(3) 0.052(3) -0.025(3) -0.002(2) -0.010(2) C36 0.038(3) 0.069(4) 0.026(3) -0.016(3) -0.006(2) -0.021(3) C37 0.031(3) 0.016(3) 0.059(4) 0.009(3) 0.002(3) -0.011(2) C38 0.023(3) 0.060(4) 0.039(3) 0.021(3) -0.003(2) -0.011(3) C39 0.062(5) 0.073(5) 0.051(4) 0.014(4) -0.001(4) 0.008(4) C40 0.084(6) 0.051(5) 0.057(4) 0.006(4) 0.020(4) -0.018(4) C41 0.059(5) 0.109(7) 0.047(4) 0.020(4) 0.015(4) 0.031(4) C42 0.071(5) 0.082(6) 0.031(3) 0.004(4) -0.003(3) -0.018(4) N1 0.025(2) 0.015(2) 0.0181(18) -0.0017(16) -0.0051(16) -0.0106(17) N2 0.0165(19) 0.015(2) 0.0137(17) 0.0007(15) 0.0004(15) -0.0081(16) N3 0.018(2) 0.0120(19) 0.0155(17) 0.0007(15) -0.0036(15) -0.0064(16) N4 0.028(2) 0.0099(19) 0.0208(19) -0.0012(16) -0.0097(17) -0.0072(17) N5 0.019(2) 0.0097(19) 0.0149(17) -0.0019(15) -0.0058(15) -0.0073(15) N6 0.018(2) 0.029(2) 0.0184(19) -0.0014(18) 0.0064(16) -0.0111(18) N7 0.034(2) 0.023(2) 0.0156(18) 0.0012(17) -0.0040(17) -0.0194(19) N8 0.032(2) 0.019(2) 0.0192(19) 0.0090(17) -0.0114(17) -0.0174(18) N9 0.020(2) 0.016(2) 0.027(2) 0.0035(17) -0.0063(17) -0.0067(17) N10 0.0155(19) 0.015(2) 0.0138(17) 0.0048(15) -0.0033(15) -0.0077(16) N11 0.028(2) 0.015(2) 0.0187(18) 0.0001(16) -0.0077(17) -0.0079(17) N12 0.051(3) 0.031(3) 0.021(2) 0.0104(19) -0.011(2) -0.031(2) O1 0.0316(19) 0.0104(16) 0.0175(15) 0.0012(13) -0.0092(14) -0.0084(14) O2 0.0316(18) 0.0099(16) 0.0184(15) 0.0015(13) -0.0108(14) -0.0095(14) O3 0.0152(16) 0.0227(18) 0.0198(15) 0.0004(14) -0.0004(13) -0.0061(14) O4 0.0183(17) 0.0178(17) 0.0179(15) 0.0006(13) 0.0024(13) -0.0065(14) O5 0.0223(18) 0.0178(17) 0.0307(17) -0.0045(15) -0.0041(14) -0.0104(14) O6 0.043(2) 0.051(3) 0.031(2) -0.0020(19) 0.0053(18) -0.015(2) Ti1 0.0193(4) 0.0104(4) 0.0129(4) 0.0020(3) -0.0028(3) -0.0060(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.327(5) . ? C1 N1 1.338(5) . ? C1 N5 1.351(5) . ? C2 N2 1.353(5) . ? C2 N11 1.356(5) . ? C2 N3 1.365(5) . ? C3 N3 1.327(5) . ? C3 N4 1.335(5) . ? C3 N5 1.351(5) . ? C4 N1 1.439(5) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 N4 1.436(5) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 N11 1.481(5) . ? C6 C7 1.511(6) . ? C6 C11 1.523(6) . ? C6 H6 1.0000 . ? C7 C8 1.514(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.519(6) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.531(6) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.505(6) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 N11 1.469(6) . ? C12 C13 1.511(6) . ? C12 C17 1.534(6) . ? C12 H12 1.0000 . ? C13 C14 1.528(6) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.515(8) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.528(7) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.523(6) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 N6 1.316(5) . ? C18 N10 1.339(5) . ? C18 N7 1.341(5) . ? C19 N7 1.355(6) . ? C19 N8 1.355(6) . ? C19 N12 1.365(5) . ? C20 N9 1.324(5) . ? C20 N8 1.336(5) . ? C20 N10 1.349(5) . ? C21 N6 1.432(6) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 N9 1.433(6) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 N12 1.458(6) . ? C23 C24 1.467(8) . ? C23 C28 1.506(6) . ? C23 H23 1.0000 . ? C24 C25 1.541(8) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.500(8) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.486(8) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.516(7) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C34 1.480(7) . ? C29 N12 1.482(7) . ? C29 C30 1.502(7) . ? C29 H29 1.0000 . ? C30 C31 1.496(8) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.548(8) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.531(7) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.498(7) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 O5 1.398(5) . ? C35 C36 1.500(7) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 O5 1.420(5) . ? C37 C38 1.498(7) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 O6 1.399(7) . ? C39 C40 1.447(8) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 O6 1.397(7) . ? C41 C42 1.451(9) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? N1 O1 1.397(4) . ? N4 O2 1.385(4) . ? N5 Ti1 2.018(3) . ? N6 O3 1.390(4) . ? N9 O4 1.395(4) . ? N10 Ti1 2.025(3) . ? O1 Ti1 1.953(3) . ? O2 Ti1 1.959(3) . ? O3 Ti1 1.965(3) . ? O4 Ti1 1.956(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 C1 N1 124.8(4) . . ? N2 C1 N5 125.0(4) . . ? N1 C1 N5 110.1(4) . . ? N2 C2 N11 116.4(4) . . ? N2 C2 N3 126.8(4) . . ? N11 C2 N3 116.7(4) . . ? N3 C3 N4 125.2(4) . . ? N3 C3 N5 125.2(4) . . ? N4 C3 N5 109.6(4) . . ? N1 C4 H4A 109.5 . . ? N1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N4 C5 H5A 109.5 . . ? N4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N11 C6 C7 112.6(4) . . ? N11 C6 C11 112.9(4) . . ? C7 C6 C11 111.7(4) . . ? N11 C6 H6 106.3 . . ? C7 C6 H6 106.3 . . ? C11 C6 H6 106.3 . . ? C6 C7 C8 110.9(4) . . ? C6 C7 H7A 109.5 . . ? C8 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 108.0 . . ? C7 C8 C9 111.4(4) . . ? C7 C8 H8A 109.3 . . ? C9 C8 H8A 109.3 . . ? C7 C8 H8B 109.3 . . ? C9 C8 H8B 109.3 . . ? H8A C8 H8B 108.0 . . ? C8 C9 C10 112.0(4) . . ? C8 C9 H9A 109.2 . . ? C10 C9 H9A 109.2 . . ? C8 C9 H9B 109.2 . . ? C10 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? C11 C10 C9 111.8(4) . . ? C11 C10 H10A 109.2 . . ? C9 C10 H10A 109.2 . . ? C11 C10 H10B 109.2 . . ? C9 C10 H10B 109.2 . . ? H10A C10 H10B 107.9 . . ? C10 C11 C6 110.9(4) . . ? C10 C11 H11A 109.5 . . ? C6 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? C6 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? N11 C12 C13 116.2(4) . . ? N11 C12 C17 113.1(3) . . ? C13 C12 C17 112.3(4) . . ? N11 C12 H12 104.6 . . ? C13 C12 H12 104.6 . . ? C17 C12 H12 104.6 . . ? C12 C13 C14 109.9(4) . . ? C12 C13 H13A 109.7 . . ? C14 C13 H13A 109.7 . . ? C12 C13 H13B 109.7 . . ? C14 C13 H13B 109.7 . . ? H13A C13 H13B 108.2 . . ? C15 C14 C13 110.7(4) . . ? C15 C14 H14A 109.5 . . ? C13 C14 H14A 109.5 . . ? C15 C14 H14B 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? C14 C15 C16 112.8(4) . . ? C14 C15 H15A 109.0 . . ? C16 C15 H15A 109.0 . . ? C14 C15 H15B 109.0 . . ? C16 C15 H15B 109.0 . . ? H15A C15 H15B 107.8 . . ? C17 C16 C15 111.0(4) . . ? C17 C16 H16A 109.4 . . ? C15 C16 H16A 109.4 . . ? C17 C16 H16B 109.4 . . ? C15 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? C16 C17 C12 109.5(4) . . ? C16 C17 H17A 109.8 . . ? C12 C17 H17A 109.8 . . ? C16 C17 H17B 109.8 . . ? C12 C17 H17B 109.8 . . ? H17A C17 H17B 108.2 . . ? N6 C18 N10 110.9(4) . . ? N6 C18 N7 124.8(4) . . ? N10 C18 N7 124.3(4) . . ? N7 C19 N8 126.8(4) . . ? N7 C19 N12 117.0(4) . . ? N8 C19 N12 116.1(4) . . ? N9 C20 N8 124.2(4) . . ? N9 C20 N10 110.6(4) . . ? N8 C20 N10 125.2(4) . . ? N6 C21 H21A 109.5 . . ? N6 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N6 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N9 C22 H22A 109.5 . . ? N9 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N9 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N12 C23 C24 115.6(4) . . ? N12 C23 C28 115.4(4) . . ? C24 C23 C28 116.0(5) . . ? N12 C23 H23 102.2 . . ? C24 C23 H23 102.2 . . ? C28 C23 H23 102.2 . . ? C23 C24 C25 112.4(5) . . ? C23 C24 H24A 109.1 . . ? C25 C24 H24A 109.1 . . ? C23 C24 H24B 109.1 . . ? C25 C24 H24B 109.1 . . ? H24A C24 H24B 107.9 . . ? C26 C25 C24 110.3(5) . . ? C26 C25 H25A 109.6 . . ? C24 C25 H25A 109.6 . . ? C26 C25 H25B 109.6 . . ? C24 C25 H25B 109.6 . . ? H25A C25 H25B 108.1 . . ? C27 C26 C25 114.7(5) . . ? C27 C26 H26A 108.6 . . ? C25 C26 H26A 108.6 . . ? C27 C26 H26B 108.6 . . ? C25 C26 H26B 108.6 . . ? H26A C26 H26B 107.6 . . ? C26 C27 C28 113.1(5) . . ? C26 C27 H27A 109.0 . . ? C28 C27 H27A 109.0 . . ? C26 C27 H27B 109.0 . . ? C28 C27 H27B 109.0 . . ? H27A C27 H27B 107.8 . . ? C23 C28 C27 111.2(4) . . ? C23 C28 H28A 109.4 . . ? C27 C28 H28A 109.4 . . ? C23 C28 H28B 109.4 . . ? C27 C28 H28B 109.4 . . ? H28A C28 H28B 108.0 . . ? C34 C29 N12 113.7(4) . . ? C34 C29 C30 115.7(5) . . ? N12 C29 C30 113.1(5) . . ? C34 C29 H29 104.2 . . ? N12 C29 H29 104.2 . . ? C30 C29 H29 104.2 . . ? C31 C30 C29 112.6(5) . . ? C31 C30 H30A 109.1 . . ? C29 C30 H30A 109.1 . . ? C31 C30 H30B 109.1 . . ? C29 C30 H30B 109.1 . . ? H30A C30 H30B 107.8 . . ? C30 C31 C32 114.2(5) . . ? C30 C31 H31A 108.7 . . ? C32 C31 H31A 108.7 . . ? C30 C31 H31B 108.7 . . ? C32 C31 H31B 108.7 . . ? H31A C31 H31B 107.6 . . ? C33 C32 C31 108.1(5) . . ? C33 C32 H32A 110.1 . . ? C31 C32 H32A 110.1 . . ? C33 C32 H32B 110.1 . . ? C31 C32 H32B 110.1 . . ? H32A C32 H32B 108.4 . . ? C34 C33 C32 113.2(5) . . ? C34 C33 H33A 108.9 . . ? C32 C33 H33A 108.9 . . ? C34 C33 H33B 108.9 . . ? C32 C33 H33B 108.9 . . ? H33A C33 H33B 107.7 . . ? C29 C34 C33 113.1(4) . . ? C29 C34 H34A 109.0 . . ? C33 C34 H34A 109.0 . . ? C29 C34 H34B 109.0 . . ? C33 C34 H34B 109.0 . . ? H34A C34 H34B 107.8 . . ? O5 C35 C36 108.1(4) . . ? O5 C35 H35A 110.1 . . ? C36 C35 H35A 110.1 . . ? O5 C35 H35B 110.1 . . ? C36 C35 H35B 110.1 . . ? H35A C35 H35B 108.4 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O5 C37 C38 108.4(4) . . ? O5 C37 H37A 110.0 . . ? C38 C37 H37A 110.0 . . ? O5 C37 H37B 110.0 . . ? C38 C37 H37B 110.0 . . ? H37A C37 H37B 108.4 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O6 C39 C40 112.0(6) . . ? O6 C39 H39A 109.2 . . ? C40 C39 H39A 109.2 . . ? O6 C39 H39B 109.2 . . ? C40 C39 H39B 109.2 . . ? H39A C39 H39B 107.9 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O6 C41 C42 110.6(6) . . ? O6 C41 H41A 109.5 . . ? C42 C41 H41A 109.5 . . ? O6 C41 H41B 109.5 . . ? C42 C41 H41B 109.5 . . ? H41A C41 H41B 108.1 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C1 N1 O1 113.2(3) . . ? C1 N1 C4 125.7(4) . . ? O1 N1 C4 115.7(3) . . ? C1 N2 C2 113.7(3) . . ? C3 N3 C2 113.3(4) . . ? C3 N4 O2 114.7(3) . . ? C3 N4 C5 127.8(4) . . ? O2 N4 C5 117.3(3) . . ? C1 N5 C3 115.8(4) . . ? C1 N5 Ti1 122.0(3) . . ? C3 N5 Ti1 122.2(3) . . ? C18 N6 O3 114.6(3) . . ? C18 N6 C21 128.2(4) . . ? O3 N6 C21 116.6(4) . . ? C18 N7 C19 114.0(4) . . ? C20 N8 C19 113.1(4) . . ? C20 N9 O4 114.2(3) . . ? C20 N9 C22 129.2(4) . . ? O4 N9 C22 116.6(3) . . ? C18 N10 C20 116.4(4) . . ? C18 N10 Ti1 121.7(3) . . ? C20 N10 Ti1 121.7(3) . . ? C2 N11 C12 122.8(3) . . ? C2 N11 C6 120.1(4) . . ? C12 N11 C6 117.0(3) . . ? C19 N12 C23 122.4(5) . . ? C19 N12 C29 120.7(4) . . ? C23 N12 C29 116.8(4) . . ? N1 O1 Ti1 120.0(2) . . ? N4 O2 Ti1 119.9(2) . . ? N6 O3 Ti1 119.7(2) . . ? N9 O4 Ti1 120.4(2) . . ? C35 O5 C37 112.2(4) . . ? C41 O6 C39 114.6(5) . . ? O1 Ti1 O4 91.12(13) . . ? O1 Ti1 O2 143.73(12) . . ? O4 Ti1 O2 95.46(13) . . ? O1 Ti1 O3 96.72(13) . . ? O4 Ti1 O3 145.82(12) . . ? O2 Ti1 O3 97.51(13) . . ? O1 Ti1 N5 73.00(13) . . ? O4 Ti1 N5 121.14(13) . . ? O2 Ti1 N5 73.11(12) . . ? O3 Ti1 N5 92.91(13) . . ? O1 Ti1 N10 110.33(13) . . ? O4 Ti1 N10 73.08(13) . . ? O2 Ti1 N10 105.70(13) . . ? O3 Ti1 N10 72.99(13) . . ? N5 Ti1 N10 165.69(15) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.932 _refine_diff_density_min -0.411 _refine_diff_density_rms 0.079